HRID2296065

反应详情

EQUATION

反应方程式

HRID 2296065 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3,0 g 1-[(p-methoxybenzyloxy)-methyl]-6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine in 30 ml of glacial acetic acid is added at 25° 24 ml 48% aqueous hydrobromic acid. The reaction mixture is stirred for 20 minutes, neutralised with 30% sodium hydroxide solution and extracted with methylenechloride. The organic phase is separated, washed with water, dried over sodium sulphate and evaporated to dryness. The crystallisation of the residue from acetate-ether-petrol ether yields 6-phenyl-8-chloro-4-H-s-triazolo[4,3-a][1,4]benzodiazepine-1-methanol, M.P. 209°-211°.

WORKUP

后处理

  1. extractionextracted with methylenechloride
  2. customThe organic phase is separated
  3. washwashed with water
  4. dry with materialdried over sodium sulphate
  5. customevaporated to dryness
  6. customThe crystallisation of the residue from acetate-ether-petrol ether